反应详情

Ethanol (0.8 mL, 13.8 mmol) was added drop wise to a stirred suspension of sodium hydride (60% dispersion in oil, 0.550 g, 13.8 mmol) in anhydrous THF (15 mL) at 0° C. and the resulting solution stirred for 0.5 hours. To this solution was added 3-fluoro-4-nitrobenzamide (2.11 g, 11.5 mmol) drop wise in anhydrous THF (15 mL). After complete addition the solution was stirred at 0° C. for 0.5 hours, before being allowed to warm to ambient temperature. The reaction was stirred at ambient temperature for 18 hours, quenched with water (30 mL) and the aqueous layer extracted with DCM (3×50 mL). The organic layers were combined, washed with brine (50 mL), dried (Na2SO4), filtered and concentrated in vacuo. The title compound was obtained as a yellow solid (1.694 g, 70% yield) after recrystallisation from MeOH.

1. additionAfter complete addition the solution
2. stirringwas stirred at 0° C. for 0.5 hours
3. stirringThe reaction was stirred at ambient temperature for 18 hours
4. customquenched with water (30 mL)
5. extractionthe aqueous layer extracted with DCM (3×50 mL)
6. washwashed with brine (50 mL)
7. dry with materialdried (Na2SO4)
8. filtrationfiltered
9. concentrationconcentrated in vacuo